反应详情

4-Aminopyridine (15.84 g) and diethyl ethoxymethylenemalonate (34.3 ml) were heated at 110° C. then allowed to stand for 16 h at room temperture. The resulting solid was collected by filtration, washed wtih diethyl ether then pentane and dried in vacuo. A sample of the resulting enamine (10.0 g) was added portionwise to refluxing Dowtherm A (400 ml ). After heating for a further 0.25 h the reaction mixture was cooled then diluted with pentane (400 ml). The precipitated solid was collected by filtration and washed wtih diethyl ether to afford the title compound as a beige solide (3.84 g).

1. filtrationThe resulting solid was collected by filtration
2. washwashed wtih diethyl ether
3. dry with materialpentane and dried in vacuo
4. additionA sample of the resulting enamine (10.0 g) was added portionwise
5. temperatureto refluxing Dowtherm A (400 ml )
6. temperatureAfter heating for a further 0.25 h the reaction mixture
7. temperaturewas cooled
8. additionthen diluted with pentane (400 ml)
9. filtrationThe precipitated solid was collected by filtration
10. washwashed wtih diethyl ether